反应详情

4-Isobutyl benzaldehyde (7 g, 0.0431 mol) is added drop wise to a mixture of concentrated sulfuric acid & nitric acid (68-72%) (9:1, 60 mL) at 0-5° C. Reaction mixture is allowed to stir at this temperature for 2 hrs, then poured into crushed ice. It is then extracted with ethyl acetate (3×40 mL). Combined organic layer is dried over sodium sulfate and concentrated under reduced pressure. The residue is purified by column chromatography (silica gel, 230-400 mesh, ethyl acetate:n-hexane 1:19) to yield 4-isobutyl-3-nitrobenzaldehyde.

1. customReaction mixture
2. additionpoured
3. custominto crushed ice
4. extractionIt is then extracted with ethyl acetate (3×40 mL)
5. dry with materialCombined organic layer is dried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue is purified by column chromatography (silica gel, 230-400 mesh, ethyl acetate:n-hexane 1:19)